缢蛏中邻苯二甲酸酯的气相色谱-质谱测定方法研究  

Study on the determination method of phthalate esters in Sinonovacula constricta by gas chromatography-mass spectrometry

作　　者：庄婉娥[1,2] 梁婧[1] 黄东仁[3] 弓振斌[1,4] 

机构地区：[1]厦门大学近海海洋环境科学国家重点实验室,福建厦门361005 [2]福建农林大学生命科学学院,福建福州350002 [3]福建省海洋环境与渔业资源监测中心,福建福州350003 [4]厦门大学环境与生态学院,福建厦门361005

出　　处：《应用海洋学学报》2013年第2期288-293,共6页Journal of Applied Oceanography

基　　金：国家海洋局海洋公益性行业科研专项资助项目(200705029)

摘　　要：建立了超声波振荡提取、固相萃取(SPE)小柱净化、气相色谱-质谱(GC-MS)同时测定缢蛏(Sinonovacula Constricta)中13种邻苯二甲酸酯(PAEs)的方法.样品用二氯甲烷超声波振荡提取和硅胶-中性氧化铝(2∶1,m∶m)固相萃取小柱对待测PAEs净化后,使用GC-MS对PAEs进行定性、定量分析.在优化实验条件下,方法的相对标准偏差(RSD)≤9.5%(20 ng/g,n=5);缢蛏样品中添加标准的回收率,除邻苯二甲酸二甲酯(DMP,58.6%)、邻苯二甲酸二乙酯(DEP,62.6%)和邻苯二甲酸二丙酯(DPRP,75.5%)偏低外,其他组分在87.9%(邻苯二甲酸丁苄酯,BBP)～111.1%[邻苯二甲酸二(2-乙基己基)酯,DEHP]之间.方法的定量检出限范围为6.3 ng/g(DMP)～32.8 ng/g(邻苯二甲酸二异丁酯,DiBP),可满足海洋生物缢蛏中痕量PAEs日常监测的需要.市售缢蛏样品中共检出3种PAEs,分别为DiBP(31.2～55.3 ng/g)、邻苯二甲酸二丁酯DnBP(39.7～51.6 ng/g)和DEHP(22.3～149.2 ng/g),与缢蛏生长环境受PAEs污染种类及PAEs理化性质有关.DEHP污染的地区差异,是样品中DEHP含量差异的原因之一.A method for accurate determination of 13 phthalate esters （PAEs）in Sinonovacula constricta, by solid phase extraction （SPE） clean-up and gas chromatography-mass spectrometry （GC-MS） detection was developed. The PAEs were first extracted with dichloromethane aided by ultrasonic cleaner, and then purified using SPE column packed with 1.0 g silica gel and 0. 5 g neuter alumina. Finally, qualitative and quantitative analyses were achieved by gas chromatography-mass spectrometry. The precisions for developed method represented by relative standard de viations （RSD）were lower than 9.5 % （20 ng/g, n = 5 ）. The standard spiked recoveries for 13 PAEs were between 87.9% （BBP） and 111.1% （ DEHP）, with the exception of DMP, DEP and DPRP which were 58.6 %, 62.6 % and 75.5 %, respectively. Limits of quantifications （LOQ） for developed method were 6.3 ng/g （DMP） - 32. 8 ng/g（DiBP）. DiBP, DnBP and DEHP were detected in the clam samples, with the concentration ranges of 31.2 - 55.3 ng/g, 39.7 -51.6 ng/g and 22. 3 - 149.2 ng/g. That was influenced by the pollutant species in environment and the physicochemical properties of PAEs. The different concentrations of DEHP in the clam samples may resulted from DEHP contaminated levels in the environment thev lived.

关 键 词：海洋化学 邻苯二甲酸酯 缢蛏 固相萃取净化 气相色谱-质谱 

分 类 号：P76[天文地球—海洋科学]